反应详情

82 g of ammonium acetate and 6.7 g of sodium cyanoborohydride were added to a solution containing 21 g of 3-(4-chlorophenoxy)-2-butanone dissolved in 500 ml of methanol, and the reaction mixture was stirred for 20 hours at room temperature. After the reaction mixture was concentrated under reduced pressure, 180 ml of concentrated hydrochloric acid, 100 ml of water, and 300 ml of diethyl ether were added to the residue. The obtained water layer was alkalified using a 5% aqueous solution of sodium hydroxide, and then the organic substances were extracted with 500 ml of ethyl acetate. The organic layer was washed with water, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. A fraction possessing a low boiling point was removed from the obtained oily products to afford 18 g (yield 86%) of the desired product.

1. concentrationAfter the reaction mixture was concentrated under reduced pressure, 180 ml of concentrated hydrochloric acid, 100 ml of water, and 300 ml of diethyl ether
2. additionwere added to the residue
3. extractionthe organic substances were extracted with 500 ml of ethyl acetate
4. washThe organic layer was washed with water
5. dry with materialdried over anhydrous magnesium sulfate
6. concentrationconcentrated under reduced pressure
7. customwas removed from the obtained oily products